肉鸡中金刚烷胺残留测定及其残留代谢规律研究

Determination of amantadine residue in broilers and study on its residual metabolism

中文关键词:  金刚烷胺  液相色谱-串联质谱法  残留分析  肉鸡

英文关键词:amantadine  liquid chromatography-tandem mass spectrometry  retention analysis  broiler

中文摘要:

      目的 建立液相色谱-串联质谱测定肉鸡中金刚烷胺残留量的分析方法, 探究鸡肉和鸡肝中的残留代谢规律。方法 样品用乙腈-乙酸-1%三氯乙酸(70:2:30, V:V:V)溶液提取, 固相萃取小柱净化后, 用液相色谱-串联质谱仪进行测定, 利用金刚烷胺-D6为内标定量。结果 金刚烷胺在0~10 μg/kg范围内线性良好, 相关系数(r2)为0.9995, 方法检测限为1 μg/kg。在添加质量浓度1~10 μg/kg范围内回收率为90.1%~95.7%, 相对标准偏差为1.17%~1.62%(n=6)。药物饲喂实验结果表明, 金刚烷胺在肉鸡中吸收快、分布广, 鸡肉中的残留明显高于鸡肝中残留含量, 鸡肉更容易产生药物蓄积。在停药13 d后, 鸡肉中金刚烷胺仍有药物蓄积, 而鸡肝中的金刚烷胺残留量为未检出。结论 该方法操作简单、灵敏度高、稳定性好, 适用于肉鸡中金刚烷胺残留的测定, 揭示金刚烷胺在肉鸡中残留代谢规律。

英文摘要:

      Objective To establish an analytical method for determining amantadine residues in broilers by liquid chromatography-tandem mass spectrometry, and explore the residual metabolism rules in chicken and chicken liver. Methods The samples were extracted with acetonitrile-acetic acid-1% trichloroacetic acid (70:2:30, V:V:V) solution. After purification by a solid-phase extraction column, the samples were determined by liquid chromatography-tandem mass spectrometry (LC-MS/MS) using amantadine-D6 as the internal standard. Results The linearity was good over the range of 0?10 μg/kg, the correlation coefficient (r2) was 0.9995, and the limit of detection of the method was 1 μg/kg. The recoveries were 90.1%?95.7% and the relative standard deviations (RSDs) were 1.17%?1.62% (n=6) within the range of 1–10 μg/kg. The results of drug feeding experiments showed that amantadine was quickly absorbed and widely distributed in broilers. The residue content in chicken was significantly higher than that in chicken liver, and chicken was more prone to drug accumulation. Drug accumulation of amantadine remained in the chicken 13 d after discontinuation and amantadine residues in the chicken liver were undetectable. Conclusion This method has the advantages of simple operation, high sensitivity and good stability, and is suitable for the determination of amantadine residues in broilers to reveal the residual metabolism of amantadine in broilers.